Manufacture of absorptive materials



Patented June 6, 1939 STATES MANUFACTURE or ABSOBP'I'IVE m'rsanms KarlJaeger, Bitter-fold, Germany, asslgnor to I.

G. Farbenlndustrie Aktiengesellschaft, Frankfort-on-the-Main, Germany INo Drawing. Application March 25, 1987. Serial No. 132,974. In GermanyApril 2, 1930 5 Claims. '(Cl. 252-2) It is known that by the action ofstrong acids, such as sulfuric acid, chlorsulfonic acid or phosphoricacid, or of zinc chloride or acid salts on organic materials, forexample wood, brown coal,

chromate or the like, and also those which in,

for exchange, give colorless, clear filtrates and.

are produced for the greater part in coarse- 5 grained condition. ,Theseproperties can be yet further improved especially when the raw materialis coal or anthracite, if the appropriate activation process is precededby treatment with organic solvents or swelling agents. It is of especialadvantage to sulfonate in the presence of a catalyst with portionsofacid of increasing concentration. Another useful method is to saturategradually the organic substance (coal etc.) mashed with the catalyst ormixture of catalysts, with gases from the contact process of makingsulfur trioxide, the rise in temperature being regulated. Thetemperature may be limited, in this novel process, to about 150 to 1600.; this ensures that the product, after separating the ex- .0 cessacid, will no longer part with constituents soluble in water or acid tothe filtrate.

The invention is illustrated by the following examples.

Example 1.-50 kilos of anthracite from which iii the fines have beenseparated together with 50 7 grams of mercury sulfate and 3 kilos ofpotassium bichromate are treated in a cast iron container, provided withmeans for heating and cooling. with 270 kilos of fuming sulfuric acidcontaining 50 20 per cent. of 80:; 180 kilos of fuming sulfuric whichmay be used for a fresh charge, is drawn oil and the solid, partiallydisintegrated product is introduced into water. It is then washed andclassified in fractions of various grain sizesby sieving. The componenthaving a grain-size of 5 between 0.2 and 0.4 mm. has a total exchangecapacity with respect to calcium chloride solution of 7.5 per cent.01:0. The component with a grain-size larger than 0.4 mm. has a capacity.lower by about one unit. 10

Example 2.--25 kilos of 'coalare sulfonated,

- under conditions similar to those described in Example 1, in thepresence of 50 grams of metcury sulfate and of 1 kilo of boric acid with12.5 kilos of fuming sulfuric. acid of 20 per cent. strength and 11kilos offuming sulfuric acid of 65 per cent. strength, the temperaturebeing limited to 140 C. The product is worked up as described in Example1, washed and sieved. The

fraction of 0.2 to 0.4 mm. size has an exchange capacity of about 7, andthe coarser fraction of about 5, per cent. (39.0. A corresponding chargewithout catalysts yields a product with an exchange value lying 1 to 2units below the figures mentioned. If, on the other hand, one attemptsto increase the activity by raising the temperature a product isobtained which usually, and especially during regeneration and duringreversal' of acid to slightly alkaline reaction. gives up a considerablequantity of colored organic matter to the filtrate.

The products obtained can be used for watersoftening and the extractionof salts, for winning metals from very weak solutions, washing outalakli and the like.

What I claim is: 1

1, The process which comprises acting upon coal with a sulfonating agentof the group consisting offsuifuric acid, fuming sulfuric acid, SO: andamidesulfonic acid in the presence of a mercury catalyst and a member ofthe group consisting of boric acid and potassium bichromate.

2. The process which comprises acting upon anthracite with a sulfonatingagent of the group consisting of sulfuric acid, fuming sulfuric acid,80:, and amidosulfonic acid in the presence of a mercury catalyst and amember of the group consisting of boric acid and potassium bichromate. i3. The processwhich comprises heating anthracite ,with fuming sulfuricacid slowly to a temperature of 150 C. in the presence of mercurysulfate and potassium bichromate.

4. The process which comprises heating anthracite with fuming sulfuricacid slowly to a temperature of 150 C. in the presence of mercurysulfate and boric acid.

5. The process which comprises treating 50 kilos of anthracite togetherwith 50 grams of mercury sulfate and 3 kilos of potassiumbichromate'w'ith 270 kilos of fuming sulfuric acid containing 20 percent. 01130:. adding gradually at a temperature up to about 150 C. 180kilos of fuming sulfuric acid containing 65 per cent. of S0: andmaintaining the temperature at 150 C. for about 2 to 3 hoiu's.

KARL JAEGER.

